Cyclic adsorption process for the recovery of ethane from a gaseous mixture consisting of methane and ethane



2 F O ym RT. ET VS OT. G S EN RO EC H July 16, 1957 E. B. MILLER CYCLIC ADSORPTION PROCESS FOR T ETHANE FROM A GAsEous MIXTURE OF METHANE ND ETHANE 6 Sheets-Sheet l Filed Jan. 16 1956 July 16, 1957 E. B. MILLER 2,799,360

CYCLIC ADSORPTION PROCESS FOR THE RECOVERY OF ETHANE FROM A GAsEouslMIxTuRE coNsIs'rfING OF METHANE AND ETHANE Filed Jan. 16, 1956 6 Sheeis-SheekI 2 FIG. 2.

INVENR" ERNEST B. MILLER ATTORNEYS July 16, 1957 E. B. MILLER 2,799,360

CYCLIC ADSORPTION PROCESS FOR THE RECOVERY F ETHANE FROM A GAsEousMIxTuRE c oNsIsTING oF METHANE` AND ETHANE Filed Jan. 1.6, 1956 v 5 Sheets-Sheet 3 //7 v //7 .f Q f y ,1f/7, f//J W IJ W. 72 l 77 l 5' 5a f 7// fafz l) i 84.. h l +8 J7 6I 7? J i d i il /y 67 @a 7 ff 2 .f2 l i Z7 ERNEST s.

ATTORNEYS July 16, 1957 E. B. MILLER CYCLIC ADSORPTION PROCESS vFOR THE RECOVERY OF ETHNE FROM A GASEOUS MIXTURE CONSISTING oF METHANE AND ETHANE 5 Sheets-Sheet 4 Filed Jan. 16, 1956 INVENTR B. M l LLER ATTORNEYS E. B. MILLER 2,799,360 ACYCLIC ADSORPTION PROCESS F OR THE RECOVERY 0F ETHNE FROM A GASEOUS MIXTURE CONSISTING A Y Y 0F IIETHANE AND ETHANE Filed Jan. 16, 195e 5` Sheets-Sheet 5 n INVENTOR .t ERNEST B. MILLER ATTORNEYS July 16, 1957 E. B. MILLER 2,799,360

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"// ATTORNEYS nited States Patent() CYCLIC ADSORPTION PROCESS FOR THE RECOV- ERY OF ETHANE FROM A GASEOUS MIXTURE CONSISTING OF METHANE AND ETHANE lErnest B. Miller, Houston, Tex., assigner to Jefferson Lake Sulphur Company, New Orleans, La., a corporation of New Jersey Application January 16, 1956, Serial No. 559,291

12 Claims. (Cl. 18S-114.2)

This invention relates to the recovery of ethane from a gaseous mixture consisting substantially of ethane and methane and has more particular reference to a cyclic process for removing and/or recovering ethane from natural gas from which substantially all constituents except ethane and methane have been removed.

One object of the present invention is to provide a novel and improved process for removing and/or recovering ethane either in liquid or gaseous form from a gaseous mixture consisting substantially of ethane and methane.

Another object of the present invention is to provide a novel process for recovering ethane from natural gas from which substantially all constituents except ethane and methane have been removed which is characterized by maintaining at least one bed of adsorbent material in each of a plurality of stages; continuously heating and recycling captive activation gas through at least one of said stages to gradually build up its concentration of desorbed products to a high concentration by volume; continuously directing a ilow of a iirst purging medium at least another one of said stages to purge the stage; continuously directing a ow of a second purging medium through at least another one of said stages to purge the stage; continuously directing the flow of the natural gas to be treated through the remainder of said stages so that substantially all of the ethane content of the gas will be adsorbed by the adsorbent material therein; periodically shifting the relative position of the particular adsorbent beds and the particular ilow of iluids in each of said stages so that each stage becomes, in succession, a first purging stage, an activation stage, a second purging stage and an adsorption stage; continuously diverting a portion of the recycling activation gas for use as the first purging medium and continuously diverting a portion of the ilow of the stripped eiiiuent natural gas from the last adsorption stage for use as the second purging medium; continuously directing the eiuent gas from the rst purging stage back into the ow of the gas being treated on its way to the adsorber; continuously directing the iiow of the etliuent gas from the second purgingstage back into the recycling activation gas; continuously withdrawing a portion ofthe captive activation gas from its recycling path after its concentration of ethane has built up to a predetermined degree, as the linished product.

Another object of the present invention is to provide a novel process for removing and/ or recovering ethane from natural gas from which substantially all constituents except ethane and methane have been removed, as characterized above, including the step of reducing the pressure of the withdrawn activation gas to a predetermined pressure and passing it through a condensing zone in which a predetermined temperature is maintained, returning the vapor phase from the condensing zone back into the recycling captive activation gas stream, and withdrawing the liquid phase from the condensing zone as the finished product.

A further object of the present invention is to provide a novel process, as characterized above, wherein the gas being treated makes two or more adsorption passages through the absorber and wherein the last adsorption passage of the gas being treated is made through freshly rc..ctivated adsorbent material.

Other objects and advantages of the invention will appear in the following specification when considered in connection with the accompanying drawings, in which:

Fig. l is a schematic View showing one embodiment of apparatus and the arrangement thereof for carrying out the method of thepresent invention and the ow of the various uids therethrough;

Fig. 2 is a side elevational view of the adsorber shown in Fig. l;

Fig. 3 is a plan View of the apparatus shown in Fig. 2;

Fig. 4 is a vertical sectional view taken on the line 4 4 of Fig. 3, but omitting the driving apparatus;

Fig. 5 is a horizontal view taken ou the line 5-5 of Fig. 4;

Fig. 6 is a fragmentary sectional view taken on the line 66 of Fig. 4, showing the manner of bracing the upper ends of the elongated adsorbent material containing vessels;

Fig. 7 is a fragmentary sectional view taken on the line 7-7 of Fig. 4, showing the manner of supporting the lower ends of the elongated adsorbent material containing vessels;

Fig. 8 is a horizontal sectional view taken on the line 8-S of Fig. 4;

Fig. 9 is a detail sectional View, taken on the line 9-9 of Fig. 8;

Fig. l0 is a vertical sectional view, with parts broken away, of the adsorbent material containing vessels shown in Fig. 4, showing the containers for holding the adsorbent material mounted therein; and

Fig. ll is a plan view 'of the container shown in Fig. l0.

The present invention provides a novel and improved process for removing and/or recovering ethane from a gaseous mixture consisting substantially of ethane and methane, such as natural gas from which substantially all constituents except ethane and methane have been removed. The process is a continuous cyclic adsorption process employing an adsorber in which at least one bed of adsorbent material is maintained iu a plurality of stages and, in general, comprises an adsorption cycle in which a continuous flow of the gaseous mixture of ethane and methane being treated is directed, under high pressure, through one or more adsorption stages so that substantially all of the ethane content of the gaseous mixture will be adsorbed by the beds of adsorbent material in the adsorption stages; an activation cycle in which a ow of captive activation gas, under high pressure, is continuously recirculated through a heater and an activation stage so that the concentration of desorbed products is built up to a high concentration by volume; a plurality of purging cycles to prevent dilution of the recycling activation gas, including a lirst purging cycle in which a portion of the activation gas is continuously diverted from its recycling path and passed into a purging stage immediately preceding the activation stage, called the first purging stage, with the eiiluent gas from the first purging stage passing into the flow of the gaseous mixture being treated on its way to the rst adsorption stage, and a second purging cycle in which a portion of the eiuent stripped gas from the last adsorption stage is continuously diverted and passed into a purging stage immediately following the activation stage, called the second purging stage, with the eiiluent gas from the second purging stage passing into the ow of the recycling activation gas; the periodical shifting of the relative positions of the particular adsorbent material and the particular flow of fluid through each stage, either by moving the beds successively through the stages or by shifting the iiows of fluid through the several stages, so that each stage becomes, in succession, a first purging stage, an activation stage, a second purging stage and an adsorption stage; and an ethane recovery cycle in which a portion of the recycling activation gas, after its concentration of desorbed products has built up to a predetermined concentration by volume, is continuously withdrawn, as the nished product.

The invention further contemplates the recovery of the iinished product in a liquid phase instead of a gaseous phase, in which case the withdrawn activation gas has its pressure reduced to a predetermined optimum pressure and is sent to a condensing and separating zone in which the temperature is maintained at a predetermined optimum degree, the vapor phase from the condensing zone is sent back to join the recycling activation gas stream and the liquid phase from the condensing zone is withdrawn as the finished product.

While any suitable usual type of adsorption apparatus may be employed to practice the process of the present invention, for purpose of illustration, the process will be described as carried out by employing a rotary type of adsorber in which a plurality of elongated upright closed vessels containing adsorbent material are rotated directly in succession and substantially continuously through the various stages of the adsorber.

Referring now to the drawings, there is shown, in Fig. l, one embodiment of apparatus and the arrangement thereof for carrying out the method of the present invention. The apparatus shown includes a seven-stage rotary adsorber 1, three stages of which are employed as adsorption stages; three stages of which are employed as purging stages; and one stage of which is employed as an activation stage; a pair of intercoolers 2 and 2 employed to cool the gas being treated between the adsorption stages; a heater 3 employed to heat the activation gas used in the activation stage; a fan or blower 4 for recirculating the activation gas through the activation stage; a fan or blower 4 for circulating the purging gas through the second and third purging stages; a pressure reducing valve 5 for reducing the pressure of the gas withdrawn from the recycling activation gas stream; a condenser separator 6 for condensing the ethane content of the withdrawn activation gas; and a compressor 5 for compressing the vapor phase from the condenser separator prior to its rejoining the recycling activation gas.

The natural gas from which substantially all constituents except methane and ethane have been removed, is delivered. at high pressure from the usual compressor or source of supply (not shown) to the first adsorption stage of the adsorber by means of a pipe line 7. The gas passes through the first adsorption stage of the adsorber, where some of the ethane is adsorbed. From the first adsorption stage of the adsorber the gaseous mixture passes through pipe line 8 and the intercooler 2 to the second adsorption stage of the adsorber. After passing through the second adsorption stage of the adsorber, where additional ethane is adsorbed, the gaseous mixture passes through pipe line 9 and intercooler 2 to the third adsorption stage of the adsorber. After passing through the third adsorption stage of the adsorber, the ethane stripped gas passes through pipe line it) to its various points of use.

The captive activation gas is heated in the heater 3 to a temperature of from 300 F. to 400 F., and from the heater passes through a pipe line 11 into the activation stage of the adsorber. The heated gas passes upwardly through the activation stage, desorbing the accumulated adsorbed ethane from the adsorbent material therein. The heated gas and the ethane desorbed from the adsorbent material pass through a pipe line i2 to the blower 4, from which they pass through pipe line 13 back to the heater 3.

The captive stream of gas in the activation system is recirculated by means or" the blower 4, through the heater 3 and the activation stage of the adsorber. This recirculation process is continuous. The recirculating captive stream of activation gas is allowed to become highly concentrated in desorbed ethane by passing directly from the activation stage outlet back to the heater without any intermediate cooling.

The vessels which contain the adsorbent beds are rotated so that each vessel passes in succession through the various stages of the adsorber. As the vessels move through each stage they are filled with the particular gas flowing through the stage and carry this gas into the next or succeeding stage in their rotary movement. This carrying of gas from one stage to the other by the vessels is called slippage.

In order to prevent the slippage gas from the tirst adsorption stage, which would consist of the gaseous mixture being treated, from being carried over into the activation stage and dilute the highly concentrated recycling activation gas, a purge stage is interposed between the first adsorption stage and the activation stage and called the first purge stage. A portion of the captive activation gas owing to the heater 3 through pipe line 13 is diverted through pipe line 13' for use as the purging gas in the first purging stage. The eiuent gas from the irst purging stage passes through pipe line 19 back into pipe line 7 to join the flow of the gas being treated on its way to the first adsorption stage of the adsorber. This permits the purging gas in the tirst purging state to push the slippage gas in the rst purging stage back into the incoming gaseous mixture being treated on its way to the first adsorption stage of the adsorber. And, as the gas used as the purging gas in the rst purging stage is obtained by continuously diverting a portion of the recycling activation gas from its recycling path, the slippage gas from the tirst purging stage into the activation stage would consist of activation gas so that the recycling captive activation gas would not be diluted.

Also, in order to prevent the slippage gas from the activation stage, which is rich in ethane, from being carried over into the third adsorption stage, where it would pass out of the adsorber with the outgoing stripped gas, two purging stages are interposed between the activation stage and the third adsorption stage, called the second purge stage and the third purge stage. Stripped gas diverted from the eiiiuent stripped gas from the third adsorption stage is employed as the purging gas for the second and third purge stages.

A portion of the efuent stripped gas flowing from the third adsorption stage of the adsorber through pipe line .ih is diverted through pipe line i7 to the blower 4', from which it passes through pipe lines i8 and 18 into the second and third purging stages, respectively, of the adsorber. The etiiuent gas from the second purging stage passes through pipe line 19 into pipe line i2., where it joins the recycling activation gas. The etiluent gas from the third purging stage passes through pipe line 19 and pipe line 19 back into the pipe line 7 to join the gas being treated on its way to the tirst adsorption stage of the adsorber.

The purging gas in the second purging stage pushes the slippage gas from the activation stage through pipe line 19' into pipe line 12, where it rejoins the recycling activation gas, while the purging gas in the third purging stage pushes the slippage gas from the second purging stage through pipe line 19" into pipe line i9 through which it passes to join the incoming stream of the gaseous mixture being treated on its way to the first adsorption stage of the adsorber. The employment of the three purging stages, as above outlined, provides for complete purging of the adsorbent material while preventing dilution of the activation gas, thus permitting the building up of a high concentration by volume of desorbed products in the recycling activation gas.

After the concentration of ethane in the recycling activation stream has reached a suitable high value, such as from about to about 93% by volume, a portion thereof is continuously diverted andf passes through pipe line 14 and the pressure reducing valve 5 therein to the condenser 6. As the gas passes through the pressure reducing valve its pressure is lowered to a predetermined value preferably between about 550 p. s. i. and about 600 p. s. i. The vapor phase from the condenser 6 passes through pipe line 15 and the compressor 5 therein back into the pipe line 12 where itV rejoins the recycling activation gas. As the vapor phase passes through the compressor its pressure is raised suficiently to permit it to ilow into pipe line 12. The liquid phase from the condenser, which is the finished product, passes through pipe line 16 to storage.

The condenser is operated at a predetermined temperature, preferably about 40 F. The pressure to which the withdrawn gas is reduced and the temperature at which the condenser is operated are determined by the concentration of ethane in the recycling activation gas stream.

When the finished product is to be recovered in gaseous form, the pipe lines 14 and 15 are closed and a portion of the recycling activation gas is withdrawn through pipe line 14' and sent to storage as the finished product.

While any suitable type of rotary adsorber may be employed to practice the method of the present invention, the adsorber illustrated is generally similar to the fluid treating apparatus shown in my co-pending application, Ser. No. 406,310, filed January 26, 1954, now Patent No. 2,751,033, dated June 19, 1956, for Fluid Treating Apparatus.

As shown in Figs. 2 to 11, inclusive, the adsorber comprises an elongated upright cylindrical pressure vessel 20 having flanged vertically aligned circular openings 21, 22 in its top and bottom walls, respectively, closed by top and bottom flanged cover plates 23, 24 removably secured to cover said openings, as by bolting; suitable framework, indicated at 25, for supporting the vessel 20 in an upright position; a rotatable vertical shaft 26 extending through the pressure vessel 20 with its upper end journaled in a suitable cap bearing carried by the upper closure member 23 and with its lower end extending through a suitable shaft seal, secured to the bottom of the lower closure member 24; a vertical shaft 27 coupled to the bottom end of the shaft 26 and connected to suitable differential gearing, indicated at 28, driven by a motor 29; a support disc 30 fixedly mounted on the shaft 26 for rotation therewith within said pressure vessel and providing support for a plurality of elongated fluid treating material containing cylindrical vessels 31; upper and lower distributive assemblages, indicated generally at 32, 33, each assemblage comprising an annular stationary member 34 having a plurality of compartments or manifolds formed therein, a tube sheet disc valve 35 slidably mounted on the shaft 26 for rotation therewith, a spring support disc 36 xedly mounted on the shaft 26 and supporting a plurality oi coiled springs 37 which engage the tube sheet disc valve 35 and tightly press it against the open end of the annular stationary member 34; a plurality of flexible pipes 38, each connecting the upper end portion of one of the vessels 31 and the tube sheet disc valve 35 of the upper distributive assemblage; a plurality of flexible pipes 39, each connecting the lower end portion of one of the vessels 31 and the tube sheet disc valve 35 of the lower distributive assemblage, a plurality of inlet-outlet conduits, seven such being shown, 40, 41, 42, 43, 44, and 46, connected to the annular stationary member 34 of the upper distributive assemblage and extending upwardly through the upper cap closure member 23, for the ingress and egress of fluids to and from the upper stationary member 34; and a plurality of inlet-outlet conduits, seven such being shown, 46', 41', 42', 43', 44', 45 and 46', connected to the annular stationary member 34 of the lower cap closure member 24- for the ingress and egress of fluids to and from the lower stationary member 34.

The cylindrical pressure vessel 20 and the cap cover members 23, 24 are preferably made of heavy boiler plate.

The flanges formed on the peripheries of the openings 21, 22 of the vessel 2t) and the peripheries of the cap cover members 23, 24 are preferably formed of heavy iron rings, rectangular in cross section and are welded to the peripheral edges of the openings and the cover plates, as indicated at 47.

The shafting 26, preferably and as shown, is formed of three sections, an upper section 48, an intermediate section 49, and a lower or bottom section 50. The upper and lower sections 48 and 50 consist of solid rod, round in cross section. The intermediate section 49 consists of a hollow pipe having an internal diameter considerably larger than the diameters of the upper and lower sections.

The upper section 48 has its upper end journalled in a suitable cap bearing 51 carried by the upper cover member 23 and its lower end supported in a support bushing 52 mounted in the upper end of the intermediate section 49 with a pin 53 passing through the two sections and the bushing fo-r rigidly and detachably securing the two sections together.

The bottom section 50 has its upper end engaged in a support bushing 54 mounted in the lower end of the intermediate section 49 with a pin 53 passing through the two sections and the bushing for rigidly and detachably securing the two sections together, and with its lower end extending through the lower cover member 24 and a suitable shaft seal 56 and coupled to the upper end of the shaft 27.

The support disc 30 which supports the cylindrical vessels 31 is composed of two semi-annular flat pieces 57, the inner adjacent straight edges of which are provided with flanges which are bolted together to form the complete disc. This is to permit of assembling the disc within the pressure vessel 20.

The disc 30 (see Figs. 4 and 7) is ixedly secured, as bolting, to a collar 58 xedly secured to the intermediate section 49 of the shaft 26, so that the disc will rotate with the shaft. The outer peripheral edge portion of the disc 30 is supported by means of a plurality of supporting links or arms 5.9, each having its upper end bolted to one of a plurality of circumferentially spaced lugs 60 carried by a collar 61 fixedly secured to the intermediate section 49 of the shaft 26 and its lower end bolted to oneof a plurality of circumferentially spaced upstanding lugs 62 secured to the upper surface of the disc 30.

The vessels 31 are supported by the disc 30, as by means of a plurality of supporting links or arms 63 in the form of short sections of structural angles, each arm 63 having its outer end portion iixedly secured to the bottom and one side of one of said vessels 31, as by welding, and its inner end portion fixedly secured, as by bolting, to one of a plurality of circumferentially spaced dependent lugs 64, in the form of short sections of l-beams, welded to the undersurface of the disc 30 (see Figs. 4 and 7).

Means may be provided for holding the cylindrical vessels 31 in their upright position encircling the shaft 26. In the particular embodiment of the invention illustrated, such means are shown as comprising a disc 65 composed of two semi-annular fiat pieces 66, 66, the inner adjacent straight edges of which are provided with flanges which are bolted together to form the complete disc. This is to permit of assembling the disc within the pressure vessel 2t). The disc 65 (see Figs. 4 and 6) is xedly secured, as by bolting, to a collar 67 xedly secured to the intermediate section 49 of the shaft 26, so that the disc will rotate with the shaft. The upper end portions of the vessels 31 are held in their upright position by the disc 65, as by means of a plurality of bracing strips or arms 68 in the form of short sections of structural angles. Each arm 68 has its outer end bolted to a lug 69 welded on the outer surface of one of the vessels 31 and its inner end portion fixedly secured, as by bolting, to the upper surface of the disc 65.

The upper and lower distributive assemblages 32, 33 are identical in construction and, as shown in Fig. 4,

each comprises an annular trough-shaped stationary member- 34 having a plurality of compartments or manifolds formed therein; a tube sheet disc valve 35 slidably mounted on the shaft 26 for rotation therewith; and a spring support disc 36 rixedly mounted on the shaft 26 and supporting a plurality of coiled springs 37 which engage the tube sheet disc valve 35 and tightly press it against the open end of the annular stationary member 34.

The upper and lower annular stationary members 34 are identical in construction and, as shown in Figs. 4, 5, 8 and 9, each is formed in the shape of an annular trough having an annular top (or bottom) wall '79 and annular side walls 7l, '72 (see Figs. 4 and 9).

The member 34 is divided into a plurality of compartments or manifolds, as by means of a plurality of circumferentially spaced pairs of wall members 73 eX- tending transversely of the member 34 and having their top (or bottom) and side walls welded to the top (bottom) and side walls of the member 34 to form gastight joints. Seven such compartments or manifolds are shown and, for the purposes of clarity of description, designated manifolds a, b, c, a', e, f and g, respectively. See Fig. S.

The upper member 3d of the upper distributive assemblage 32 is held stationary relative to the rotation of the shaft 2o and the upper tube sheet disc valve 35 by the upper inlet-outlet conduits 4t), 41, 42, 43, 44, Ll5 and 46, which are welded to the upper cap closure member 23 and have their lower ends connected, as by welding, to manifolds a, b, c, d, e, f and g, respectively, in the upper member 34 to provide communication therewith.

The lower member 34 of the lower distributive assemblage is held stationary relative to the rotation of the shaft 2.6 and the lower tube sheet disc Valve 35 by the lower inlet-outlet conduits 49', 4l', 42', 43', 44', 45', and 46', which are welded to the lower cap closure 24 and have their upper ends connected, as by welding, to the manifolds rz, b, c, d, e, f and g, respectively, in the lower member 34!- to provide communication therewith.

The upper and lower tube sheet disc valves 35 are identical in construction and, as shown in Fig. 4, each comprises a flat metal disc having a plurality of circumferentially spaced circular openings '74 formed in a circular row adjacent its periphery. The disc is provided with a collar 75' having a plurality of radially extending reinforcing ribs welded to its bottom surface or cast integral therewith. The collar 75 is lieyed on the upper (lower) section of the shaft 26 to have longitudinal movement therealong as well as rotative movement therewith, as by means of a set screw 76 slidably engaging in a longitudinal groove 77 formed in the upper (lower) section of the shaft 26. A second collar 78 is xedly secured to the shaft 25 immediately beneath the collar '75 to limit the inward movement of the disc as it moves longitudinally of the shaft 2e. The disc 35, as well as the collar 75, are loosely tted on the shaft 2o so that the disc valve can be moved slightly to conform to any change in the plane of the engaged surface of the stationary member 3d, due to unequal expansion and contraction.

The tube sheet disc 35 is so mounted on the shaft 25 that it slidably engages the open bottom (top) end of the annular stationary member 34 with the circular row of openings 7d vertically aligned with the manifolds a, b, c, d, e, f and g, so that each manifold will be in communication with a group of the circular openings.

The upper and lower' spring support discs 36 are identical in construction and, as shown in Fig. 4, each comprises a metal disc mounted on the shaft and having a hub 79 provided with a plurality of circumferentially spaced radial ribs or webs welded to the under face of the disc to strengthen it. The hub is Xedly secured to the shaft, as by a set screw. A plurality of vertically eX- tending circumferentially spaced coiled springs 37 are interposed between the tube sheet disc valve 35 and the spring support disc 36. In order to insure that the springs 37 remain in proper position7 they are mounted on and between short stubs 8d extending upwardly from the disc 36 and short corresponding stubs Sil' extending downwardly from the disc 35. The construction and arrangement is such that the springs 37 will keep the dise valve 35 evenly and rrnly pressed into engagement with the under surface of the annular stationary member 34.

The upper and lower flexible pipes 38, 39, which connect the upper and lower end portions of the adsorbent material containing vessels 31 to the upper and lower distributive assemblages are identical in construction and, as shown in Figs. 4 and l0, each comprises a thin walled cylindrical metal tube having the greater portion of its wall formed in a sinuous shape to give it flexibility, the outer cylindrical end of each tube is detachably secured to a nozzle Sl formed on the upper (lower) end portion of the vessel 3l, as by strapping. The cylindrical inner end of the tube is provided with an integral flange 82. The opening in the cylindrical inner end of the tube is aligned with one of the circular openings "iii formed in the upper (lower) tube sheet disc valve 35 and the flange 32 is detachably secured to the outer surface of the disc valve, as by countersunk bolts, so that the inner surface of the disc wall will be smooth and uninterrupted (see Fig. 4).

To prevent the escape of gas between the rotating tube sheet disc valve 3S and the manifolds in the member 34, sealing ring gaskets 83 are placed at the juncture of the side walls of the member 34 and the disc valve 3S. The ring gaskets 83 are wedged into annular troughs 34, secured, as by welding, to the outer surface of the side walls of the member 34. Each trough comprises an annular top (bottom) wall 85 and an annular side wall 86. The ring gaskets 83, preferably and as shown, cornprise a plurality of annular strips of packing, generally rectangular in cross section and made of any suitable material, such as Teon impregnated asbestos.

The seven manifolds a, b, c, d, e, f and g are sealed olf from each other by means of cross seals 87, each sealed into a recess 83 formed by the adjacent end walls of the manifolds and a bottom plate 89 vertically spaced from the open end of the manifolds (see Figs. 8 and 9). Each cross seal is tightly wedged in its recess with its outer ends in tight engagement with the adjacent side walls of the annular seals S3 and with its bottom surface in sealing engagement with the upper (lower) surface of the tube sheet disc. In order for the outer ends of the cross seals to engage the adjacent side Walls of the annular seals 53, the portions of the side walls 71 and 72 of the member 34 which extend between each pair of adjacent transverse members 73 are cut away, as indicated at 90, for a distance equal to the thickness of the seals S3 (see Fig. 9).

The widths of the manifolds a, b, c, d, e, f and g are substantially the same as the internal diameters of the circular openings 74 in the tube sheet disc 35, so that each cross seal can effectively seal off one of the openings.

Each of the openings 74 formed in the upper tube sheet disc 35 is in vertical alignment with a corresponding one of the openings '74 formed in the lower tube sheet disc 35 and each of the cross seals 37 which separate the manifolds a, b, c, d, e, f and g formed in the upper stationary member 34 is in vertical alignment with a corresponding one of the cross seals 87 which separate the manifolds a, b, c, d, e, f and g formed in the lower stationary member 34.

When the rotary disc valves 35 and the vessels 31 are stationary, the foregoing ar-rangement, in effect, divides the adsorbent material containing vessels 31 into seven groups, with one group connected to communicate with the manifolds a, one group connected to communicate with the manifolds b, one group connected to communicate with the manifolds c, onev group connected to communicate with the manifolds d, one group connected to communicate with the manifolds e, one group connected to communicate with the manifolds f, and one group connected to communicate with the manifolds g. Each group of vessels 31, together with the upper and lower manifolds with which they are in communication form separate llow passages through the adsorber so that seven separate, distinct and continuous llows of fluid may pass through the apparatus. Each ilow entering the upper distributive assemblage by means of one of the inletoutlet conduits 40, 41, 42, 43, 44, 45, or 46, thence through one of the groups of vessels 31 into the lower distributive assemblage and out through one of the inletoutlet conduits 40', 41', 42', 43', 44', 45', or 46. As the vessels 31 and the upper and lower disc valves 35 rotate, each of the flows of iluid will successively pass through the vessels 31. For convenience in description, each llow passage is called a stage, in which either adsorption, activation, or purging takes place, depending upon the particular fluid llowing therethrough. Also, the vessels 31 are called zones, in which either adsorption, activation or purging takes place, depending upon the particular fluid owing therethrough at a given time.

The adsorbent containing vessels 31 are identical in construction and, as shown in Figs. l() and ll, each comprises an elongated hollow tubular member 91 having a closed bottom end and an open upper end provided with a flanged collar 92 to which is secured, as by bolting, a removable cover plate 93.

A horizontally disposed annular disc 94 is mounted in the lower end portion of the member 91 and secured therein, as by welding, to form a gas-tight joint between the outer peripheral edge of the disc and the side wall of the member 91. The lower annular disc 94 forms a support for an elongated annular fluid treating material container 95. The container 95 is removably mounted within the member 91, with its bottom end resting on the annular disc 94 and with the longitudinal open end of the container aligned with the opening in the disc.

The tubular member 91 has a tapered side wall for a purpose hereinafter to be described and is provided with upper and lower circular openings 96 in which are secured, as by welding, the nozzles 81 to which the upper and lower flexible pipes 38 and 39 are secured.

A baille member 97 is mounted in the space between the bottom of the member 91 and the annular disc 94, and an upper baille member 98 is secured to the underside of the cover plate 93 and is removable therewith. The upper and lower baille members 98 and 97 are identical in construction and, as shown in Fig. l0, each comprises a generally elliptical-shaped ilat sheet 99 eX- tending upwardly (downwardly) from the bottom (top) of the member 91 to insure an even flow of fluid through the member 91; a side wall forming member 100; and insulating material 101 placed within the pocket formed by the members 99 and 100 and the bottom (top) wall of the member 91 (see Fig. 10).

The containers 95 are identical in construction and, as shown in Figs. l and, ll, each comprises two concentric tubular screens 102, 103, held in spaced-apart relation by a plurality of longitudinal radial ns 104,*with the annular space between the screens closed at the bottom,- as by a flanged annular plate 105. The mesh of the screens is such as to retain a granular adsorbent material 106 in the annular space between the screens. In the instant case, the adsorbent material may be of any adsorbent having characteristics substantially like silica `gel or the gel of other activated hydrous oxides. Preferably silica gel is used. v

Each of the containers 95 is closed at its top by means of concentric hoops or metal bands 107, 108 mounted on the concentric screens 102, 103, and a cover plate 109 is detachably connected to the inner hoop or band 108, as by screws, and having a depending annular flange 110 fitting between the hoops or bands 107, 108. A depend- 10 ing'cylindrical n 111 is secured to the flange 110 and projects downwardly between and below the hoops or bands 107, 108, and lits in slits 112 formed in the upper ends of the radial ns 104, all as shown in Figs. l0 and 1l. The construction is such that, as the silica gel settles down, leaving a space between the top portion of the wire lscreens devoid of silica gel, the tins 111 will prevent lluid from passing through the space.

Mounted within the inner wire screen 103 is an inverted substantially conically shaped baille member 113. The baffle member 113 is closed at its apex which extends downwardly to a point near the bottom of the container and has its upper peripheral edge suitably secured to the band 108, as by welding. Preferably, the baffle member 113 is made of thin sheet metal.

When the container is mounted within the hollow member 91, as shown in Fig. l0, the elongated annular space between the walls of the member 91 and the inverted conical baille member 113 forms an elongated frustoconically shaped duct which is annular in cross section. The annular container, filled with silica gel, is positioned in the duct between the members 91 and 113 in such manner that it forms a barrier extending longiudinally across the duct from top to bottom. The cross sectional areas of the duct at its top and bottom are substantially equal and the tapers of its side walls are such that a substantially uniform velocity is obtained on both sides of the barrier as lluid is transferred from the upstream to the downstream side, regardless of the direction of llow, thereby creating a substantially constant static head over the face of the barrier, resulting in a substantially uniform distribution of the fluid throughout the entire barrier area. Thus, it will be seen that by using the members 91 and 113, as baffle members, the entire area is made use of with resultant increase in efficiency, capacity and economy.

Means may be provided so that the containers 95 which hold the adsorbent material may readily be removed from and replaced in the vessels 31. As shown, such means may comprise an opening 114 formed in the top of the top of the vessel 20 having a cylindrical member 115 welded therein and provided with a readily removable closure disc 116 secured in the upper end of the member 115, as by means of a split shear ring 117 bolted thereto and tted into a circumferential recess 118 formed in the inner surface of the member 115, and an O-ring packing 119 mounted between the closure disc 116 and the side wall of the member 113 to insure gas tightness.

The flows of the various gases through the various stages of the adsorber and the auxiliary apparatus are schematically shown in Fig. 1.

As there shown, the natural gas from which substantially all constituents except methane and ethane have been removed, is supplied under high pressure from about 800 vp. s. i. to about 1000 p. s. i. by pipe line 7 and enters manifold a of the upper distributive assemblage through inlet-outlet conduit 40. From manifold a the gas passes through openings 74 formed in the upper tube sheet disc valve 35 and flexible pipes 3S into the upper end portion of the group of vessels 31 which are at that time in communication with the manifold a. The gas passes down through the silica gel beds therein into the bottoms of the vessels. The baille members 113, in cooperation with the tapered side walls of the Vessels 31, insure a substantially uniform flow and distribution of the gas through the silica gel beds, which adsorb some of the ethane content from the gas. From the bottoms of the vessels 31, the now partially ethane stripped gas passes through outlet pipes 39 and openings 74 in the lower tube sheet disc valve 35 into the manifold a of the lower distributive assemblage.

From the lower manifold a of the lower distributive assemblage, the gas passes through inlet-outlet conduit 40 and pipe line Sand intercooler 2 to the second adsorption stage and enters manifold b of the lower distributive assemblage through inlet-outlet conduit 41'. From the lower manifold b the gas passes through openings 74 in the tube sheet disc valve 35 and inlet pipes 39 into the lower end portion of the group of vessels 31 which are at that time in communication with manifold b. The gas passes upwardly through 'the vessels 31 of the second group and through the silica gel beds therein into the tops thereof, additional ethane being adsorbed from the gas during its passage through the silica gel beds.

From the tops of the vessels 31 of the second adsorption group, the gas passes through pipes 38 and openings 74 in thel upper tube sheet disc valve of the upper distributive assemblage into the upper manifold b.

From the upper manifold b the gas passes through inlet-outlet pipe 41 and pipe line 9 and intercooler 2 to the third adsorption stage and enters upper manifold c of the upper distributive assemblage through inlet-outlet conduit 42.

From the upper manifold c the gas passes through openings 74 in the tube sheet disc valve 35 and inlet pipes 38 into 'the upper end portions of the group of vessels 31 which are at that time in communication with manifold c. The gas passes downwardly through the vessels 3l of the third group and through the silica gel beds therein into the bottoms thereof. The remaining ethane content of the gas being adsorbed during its passage through the silica gel beds.

Frm the bottoms of the vessels 3l of the third group, the gas passes through pipes 39 and openings 74 in the tube sheet disc valve 35 into the lower manifold c. From the lower manifold c the gas passes through inletoutlet conduit 42 and pipe line lil to the various points of use.

The removal and recovery of the ethane from the beds of adsorbent material is effected in the activation stage. The activation gas, a captive gas, is heated in a heater 3, where its temperature is raised to from 250 F. to 400 F. From 'the heater, the heated activation gas passes through pipe line il and inlet-outlet conduit 45 into the lower manifold f of the lower distributive assemblage. From the manifold f the hot activation gas passes through openings 7din the lower tube sheet disc valve 35 and flexible pipes 3g into the lower end portions of the groups of vesseis 31 which are at that time in communication with manifold f. The gas passes upwardly through vessels 3l of the activation group and through the silica gel beds therein into the tops thereof. As the hot gas passes lthrough the adsorbent material it removes the adsorbed ethane therefrom. From the tops of the vessels 3l, the hot ethane laden gas passes through flexible pipes 33 and openings 74 in the lower tube sheet disc valve 35 into the upper manifold f. From the upper manifold f, the hot gas passes through inlet-outlet conduit i5 and pipe line 12 to the blower 4 and is recycled by the blower through pipe line i3 and the heater 3, back through the activation stage. This recirculation process is continuous.

The recirculating captive stream of activation gas is allowed to become highly concentrated in desorbed products by passing directly from the activation stage outlet back to the heater without any intermediate coolmg.

After the concentration of ethane in the recycling activation gas has reached a predetermined value of from about 83% to about 93% by volume7 a portion thereof is continuously diverted and passes through pipe line i4 the pressure reducing valve 5 therein to the condenser 6. As the gas passes through the pressure reducer the pressure is lowered to a predetermined pressure, preferably between from about 550 p. s. i. to about 600 p. s. i. The liquid phase from the condenser, which is the finished product, passes through pipe line 16 to storage. The vapor phase from the condenser passes through pipe line l5 and the compressor 5 therein, where its pressure is raised to a pressure equal to or greater than the pressure of the recycling activation gas, back into pipe line 12, where it rejoins the recycling activation gas. In some instances, it may be desirable to recover the finished product in a gaseous phase instead of a liquid phase. This can be accomplished by closing the stop valves in the pipe lines 14 and l5 to cut out the pressure reducer 5, the condenser 5, and the compressor 5 and opening the stop valve in a pipe line 14' connected to the pipe line 12.

In order to prevent slippage of activation gas, rich in desorbed products, into the outgoing stripped gas, and in order to prevent dilution of the highly concentrated activation gas, a first purging stage is provided ahead of and a second and third purging stage are provided following the activation stage.

A portion of the recycling activation gas is diverted from pipe line 13 for use as the purging gas in the first purging stage and passes through pipe line 13 and inletoutlet conduit 46 into the lower manifold g of the lower distributive assemblage. From the manifold g the purging gas passes through openings 74 in the lower tube sheet disc valve 35 and flexible pipes 39 into the lower portions of the group of vessels 31 which are at that time in communication with manifold g. The gas passes upwardly through the vessels 31 of the first purging stage and through the silica gel beds therein into the tops thereof. As the purging gas passes through the adsorbent material it removes the slippage natural gas, thereby purging the beds. From the tops of the vessels 31 the eilluent gas consisting substantially of slippage gas from the first adsorption stage passes through flexible pipes 3S and openings '74 in the upper tube sheet disc valve 35 into the upper manifold g. From the upper manifold g the gas passes through inlet-outlet conduit 46 and pipe line 19 back into pipe line 7 and joins the natural gas being treated on its way to the adsorber.

The gas used as the purging gas in the second purging stage is obtained by continuously diverting a portion of the flow of the stripped natural gas through pipe line 10 from the last adsorption stage of the adsorber through pipe line 17 to the blower 4. From the blower 4' the purging gas passes through pipe line 18 and inlet-outlet conduit 44 into the lower manifold e of the lower distributve assemblage. From the manifold e the purging gas passes through openings 74 in the lower tube sheet disc valve 35 and flexible pipes 39 into the lower end portions of the group of vessels 31 which are at that time in communication with manifoldk e. The gas passes upwardly through the vessels 31 of the second. purging group and through the silica gel beds therein into the tops thereof. As the purging gas passes through the adsorbent material it removes any remaining activation gas or deposited vapors therefrom, thereby purging the beds. From the tops of the Vessels 31, the eilluent gas consisting substantially of slippage activation gas passes through flexible pipes 38 and openings 74 in the upper tube sheet disc valve 35 into the upper manifold e. From the upper manifold e the gas passes through inlet-outlet conduit 44 and pipe line 19' into pipe line 12 and joins the recycling activation gas.

A portion of the purging gas flowing through pipe line 18 is diverted and passes through pipe line 18 and inletoutlet conduit 43 into manifold d of the lower distributive assemblage. From the manifold d the purging gas passes through openings 74 in the tube sheet disc valve 35 and inlet pipes 39 into the lower endl portion of the group of vessels 31 which are at that time in communication with manifold d. The gas passes upwardly through the vessels 31 of the third purging group and through the silica gel beds therein into the top thereof. The purging gas removes any remaining activation gas and purges the silica gel beds during its passage through the beds of the third purging stage.

From the tops of the vessels 31 of the third purging stage the eluent gas consisting substantially of slippage pipes 38 and openings 74 in the upper tube sheet disc valve of the upper distributive assemblage into the upper manifold d. From the manifold d the gas passes through inlet-outlet conduit 43, pipe line 19", 'and pipe line 19 to join the gas being treated flowing through pipe line 7 on its way to the adsorber.

The gas being treated makes three passes through the adsorber, while the activating gas and each of the purging gases each make a single pass through the adsorber. For convenience in description, the stage of the adsorber through'which the first adsorption passage of the .gas being treated is made, is called the rst adsorption stage, the stage through which the second adsoption passage is made is called the second adsorption stage, the stage through which the third adsorption passage is made is called the third adsorption stage, the stage through which the hot gas used for activation passes is called the activation stage, the stage through which the first purging gas passes is called the first purging stage, the stage through which the second purging gas passes is called the second purging stage, and the stage through which the third purging gas passes is called the third purging stage. Also, the vessels 31 are called zones in which either adsorption, activation, or purging takes place, depending upon the particular fluid fiowing therethrough at a given time. In addition, the condenser separator 6 is called a condensing and separating zone or stage and the heater 3 is called a heating zone.

In the particular embodiment of the invention illustrated, the valve discs 35 and the vessels 31 are rotated clockwise, as viewed in Fig. 2, and at a rate such that the efliuent gas tiow from the purging stages will be substantially volumetric with the slippage gas brought into these stages as the vessels 31 are rotated; thus it will be seen that, as the valves 35 and the vessels 31 rotate, each of the vessels 31 will be successively brought into communication with the manifolds g, f, e, d, c, b and d in the upper and lower distributive assemblages, so that each vessel 31 will, in turn, become a first purging zone, an activation zone, a second purging zone, a third purging zone, a third adsorption zone, a second adsorption zone, and a first adsorption zone.

Suitable stop valves are provided at any desiredpoint in any pipe line to provide means for controlling the flow of the various mediums through the various stages of the adsorber and the auxiliary apparatus.

From the foregoing, it readily will be seen that there has been provided a novel and improved method of removing and recovering ethane from a gaseous mixture consisting substantially of methane and ethane such as natural gas from which substantially all of its constituents except methane and ethane have previously been removed; an improved method which eliminates slippage of the activation gas into the outgoing stripped gas, and returns the natural gas being treated contained in the vessels 31 as they enter the activation stage, back to the natural gas stream on its way to the adsorber thereby preventing dilution of the activation gas.

While some of the flows of fluid through the apparatus have been described as entering the top distributive assemblage and flowing downward to and out of the bottom distributive assemblage, obviously, the flows may be in either direction.

Obviously, too, the present invention is not restricted to the particular embodiment thereof herein shown and described.

What is claimed is:

l. A method of removing and recovering ethane from a gaseous mixture consisting substantially of methane and ethane comprising rotating a series of separated beds of adsorbent material directly in succession and substantially continuously relative to and through a first purging stage, an activation stage, a second purging stage, and at least one adsorption stage; continuously directing a 14 flow of the gas to be treated under high pressure and in succession through the ladsorption stages so that the ethane content thereof will be adsorbed by the adsorbent material therein; continuously recycling a flow of captive activation gas through a heating Zone and there heating the captive gas, then directly through'said activation stage lto desorb theethane contained in the beds of adsorbent material therein, then directly back to said heating zone, whereby the recycling captive activation gas will become highly concentrated in desorbed ethane; continuously diverting a portion of the recycling activation gas for use as the purging gas for the first purging stage and directing its tiow into the first purging stage and continuously directing the iiow of the eliiuent gas from the first purging stage into the flow of the gas being treated on its way to the first adsorption stage; continuously directing a portion of the stripped effluent gas from the last adsorption stage for use as the second purging gas and directing its flow into the second purging stage and continuously directing the flow of the effluent gas from the second purging stage into the ow of the captive recycling activation gas on its way to be heated; and'continuously withdrawing a portion of the activation gas from its recycling path after it has become highly concentrated in ethane to a predetermined 2. The method as set forth in claim 1, including reducingrthe pressure of the portion of withdrawn activation gas to a predetermined pressure, then sending it to a condensing zone in which a predetermined temperature is maintained to condense the ethane therein, and withdrawing the liquid phase from the condensing zone as the finished product.

3. The method as set forth in claim 2, including withdrawing the vapor phase from the condensing zone, raising its pressure and returning it to the recycling activation gas stream.

4. A method of recovering ethane from a gaseous mixture consisting substantially of methane and ethane comprising maintaining at least one bed of adsorbent material in each of a plurality of zones; continuously recycling a tiow `of captive activation gas under high pressure through a heating zone and there heating the captive gas, then directly through at least one of said zones to desorb the ethane contained in the adsorbent material therein, then directly back to said heating Zone whereby the recycling captive activation gas will become highly concentrated in desorbed ethane; continuously directing a first liow of a purging medium under high pressure through at least another one of said zones to purge the zone; continuously directing a second liow of a purging medium under high pressure through at least another one of said zones to purge the zone; continuously directing the liow 0f the gas being treated under high pressure through the remainder of said zones so that the ethane 4content of the gas will be adsorbed by the adsorbent material therein; periodically shifting the relative positions of the particular adsorbent material and the particular flow of fluid in each of said zones so that each zone becomes in succession a first purging zone, 'an activation Zone, a second purging zone and an adsorption zone; continuously diverting a portion of the recycling activation gas for use as the first purging medium and continuously directing the fiow of the efiiuent gas from the first purging zone into the tiow of the gas being treated on its way to the first adsorption zone; continuously diverting a portion of the stripped efliuent gas from the last adsorption zone for use as the second purging medium and continuously directing the flow of the effluent gas from the second purging Zone into the iiow of the recycling captive activation gas; and continuously withdrawing a portion of the activation gas from its recycling path, after it has become highly concentrated in desorbed ethane as the finished product.

5. The method as set forth in claim 4, including reducing the pressure of the portion of Withdrawn activation gas to a predetermined pressure, then sending it to a degree by volume, as the finished product,v

condensing zone in which a predetermined temperature is maintained to condense the ethane therein, and Withdrawing the liquid phase from the condensing zone as the finished product.

6. The method as set forth in claim 5, including withdrawing the vapor phase from the-condensing zone, raising its pressure and returning it to the recycling activation gas stream.

7. A method of recovering ethane from natural gas from which substantially all constituents have been removed except ethane and methane comprising rotating a series of separated beds of adsorbent material directly in succession and substantially continuously relative to and through a first purging stage, an activation stage, a second purging stage, a third purging stage, and a plurality of adsorption stages; continuously directing a ilow of the gas to be treated under high pressure in succession through said adsorption stages so that the ethane content of the gas will be adsorbed by the adsorbent material as it passes through said adsorption stages; recycling a flow of captive activation gas through a heating zone and there heating the captive gas, then directly through said activation stage, then directly back to said heating zone until the concentration of desorbed ethane in said captive gas has reached to from about 80% to about 93% by volume; continuously recycling said highly concentrated captive gas stream through said heating zone and said activation stage; continuously diverting a portion of the activation gas from its recycling path and directing its llow through the first purging stage and continuously directing the flow of the effluent gas from the first purging stage into the flow of the natural gas on its Way to the first adsorption stage of the adsorber; continuously diverting a portion of the flow of the eflluent stripped gas from the last adsorption stage and directing its ow through the second and third purging stages; continuously directing the flow of` the efuent gas from the second purging stage into the recycling activation gas; continuously directing the ow of the efuent gas from the third purging stage into the flow of the natural gas on its way to the first adsorption stage; continuously withdrawing a portion of the activation gas from its recycling path after it has become highly concentrated with desorbed ethane, as the finished product.

8. The method as set forth in claim 7 including reducing the pressure of the portion of withdrawn activation gas to a predetermined pressure then sending it to a condensing zone in which a predetermined temperature is maintained to condense the ethane therein, and with- L.

drawing the liquid phase from the condensing zone as the finished product.

9. The method as set forth in claim 8 including the step of withdrawing the vapor phase from said condensing zone, raising its pressure and returning it to the recycling activation gas stream.

l0. A method of recovering ethane from natural gas,-

l tive `activation gas under high pressure through a heating zone ,and there heating the captive gas, then directly through at least one of said zones to desorb the ethane contained in the adsorbent material therein, then directly back to said heating zone whereby the recycling captiveV activation gas will become highly concentrated in desorbed ethane; continuously directing a rst flow of a purging medium under high pressure through at least another one of said zones to purge the zone; continuously directing a second flow of a purging medium under high pressure through at least another one of said zones to purge the Zone; continuously directing a third flow of a purging medium under high pressure through at least another one of said Zones to purge the zone; continuously directing the flow of the gas being treated under high pressure through the remainder of said zones so that the ethane content of the gas will be adsorbed by the adsorbent material therein; periodically shifting thev relative positions of the particular adsorbent material and the particular flow of fluid in each of said zones so that each zone becomes in succession a first purging zone, an activation zone, a second purging zone, a third purging zone, and an adsorption zone; continuously diverting a portion of the recycling activation gas for use as the first purging medium and continuously directing the flow of the effluent gas from the first purging Zone into the f'low ofthe gas being treated on its Way to the rst adsorption zone; continuously diverting a portion of the flow of the stripped effluent gas from the last adsorption zone for luse as the purging medium for the second and third purging zones; continuously directing the flow of the effluent gas from the seco-nd purging zone into the ow of the recycling captive activation gas; continuously directing the flow of the eluent gas from the third purging zone into the flow of the gas being treated on its way to the first adsorption zone; and continuously withdrawing a portion of the activation gas from its recycling path, after it has become highly concentrated in desorbed ethane, as the finished product.

1l. The method as set forth in claim 10 including reducing the pressure of the portion of withdrawn activation gas to a predetermined pressure, then sending it to a condensing zone in which a predetermined temperature is maintained to condense the ethane therein, and withdrawing the liquid phase from the condensing zone as the nished product.

l2. The method as set forth in claim 11, including withdrawing the vapor phase from the condensing zone,

raising its pressure and returning it to the recycling activation gas stream.

References Cited in the file of this patent UNITED STATES PATENTS 1,721,033 Okochi July 16, 1929 1,998,774 Bulkeley Apr. 23, 1935 2,495,842 Gilliland Ian. 3l, 1950 2,507,608 Miller May 16, 1950 2,739,669 Miller Mar. 27, 1956 2,739,670 Miller Mar. 27, 1956 

1. A METHOD OF REMOVING AND RECOVERING ETHANE FROM A GASEOUS MIXTURE CONSISTING SUBSTANTIALLY OF METHANE AND ETHANE COMPRISING ROTATING A SERIES OF SEPARATED BEDS OF ADSORBENT MATERIAL DIRECTLY IN SUCCESSION AND SUBSTANTIALLY CONTINUOUSLY RELATIVE TO AND THROUGH A FIRST PURGING STAGE, AN ACTIVATION STAGE, A SECOND PURGING STAGE, AND AT LEAST ONE ADSORPTION STAGE; CONTINUOUSLY DIRECTING A FLOW OF THE GAS TO BE TREATED UNDER HIGH PRESSURE AND IN SUCCESSION THROUGH THE ADSORPTION STAGES SO THAT THE ETHANE CONTENT THEREOF WILL BE ADSORBED BY THE ADSORBENT MATERIAL THEREIN; CONTINUOUSLY RECYCLING A FLOW OF CAPTIVE ACTIVATION GAS THROUGH A HEATING ZONE AND THERE HEATING THE CAPTIVE GAS, THEN DIRECTLY THROUGH SAID ACTIVATION STAGE TO DESORB THE ETHANE CONTAINED IN THE BEDS OF ADSORBENT MATERIAL THEREIN, THEN DIRECTLY BACK TO SAID HEATING ZONE, WHEREBY THE RECYCLING CAPTIVE ACTIVATION GAS WILL BECOME HIGHLY CONCENTRATED IN DESORBED ETHANE; CONTINUOUSLY DIVERTING A PORTION OF THE RECYCLING ACTIVATION GAS FOR USE ING ITS FLOW INTO THE FIRST PURGING STAGE AND CONTINUOUSLYNG DIRECTING THE FLOW OF THE EFFUENT GAS FROM THE FIRST PURGING STAGE INTO THE FLOW OF THE GAS BEING TREATED ON ITS WAY TO THE FIRST ADSORPTION STAGE; CONTINUOUSLY DIRECTING A PORTION OF THE STRIPPED EFFUENT GAS FROM THE LAST ADSORPTION STAGE FOR USE AS THE SECOND PURGING GAS AND DIRECTING ITS FLOW INTO THE SECOND PURGING STAGE AND CONTINUOUSLY DIRECTING THE FLOW OF THE EFFUENT GAS FROM THE SECOND PURGING STAGE INTO THE FLOW OF THE CAPTIVE RECYCLING ACTIVATION GAS ON ITS WAY TO BE HEATED; AND CONTINUOUSLY WITHDRAWING A PORTION OF THE ACTIVATION GAS FROM ITS RECYCLING PATH AFTER IT HAS BECOME HIGHLY CONCENTRATED IN ETHANE TO A PREDETERMINED DEGREE BY VOLUME, AS THE FINISHED PRODUCT. 